摘要
研究了在卵类糖蛋白(OGCH I)手性柱上影响钙离子拮抗剂尼卡地平对映体拆分的主要因素,建立了尼卡地平对映体的拆分方法。氨丙基硅胶在0.2 mol/L磷酸钠缓冲液(pH 6.6)中与OGCH I反应,制备的固定相装填于10 cm不锈钢柱中,用高效液相色谱法拆分尼卡地平对映体。优化的色谱条件为:0.05 mol/L磷酸钠缓冲液(pH 5.5)-甲醇(65∶35),流速0.2 mL/m in,紫外检测波长236 nm,柱温:25℃。在此条件下,尼卡地平对映体可得到良好分离。通过改变有机改性剂的种类和比例、流动相的pH值、缓冲溶液的浓度以及流速等色谱条件,确定了影响尼卡地平对映体拆分的主要因素。
A high performance liquid chromatography (HPLC) method for the enantiomeric separation of nicardipine was established by using ovoglycoprotein as stationary phase. Aminopropylsilica gels were reacted with ovoglycoprotein in 0.2 mol/L sodium phosphate buffer and packed into a stainless steel column. Baseline separation of nicardipine enantiomers was achieved on the column with a mobile phase consisted of 0.05 mol/L sodium phosphate buffer ( pH 5.5 ) -methanol ( 65 : 35 ) at a flow rate of 0.2 mL/min, and detection at the wavelength of 236 nm. The column temperature was fixed on 25℃. The influence of the organic modifier type and concentration, pH of the mobile phase, the buffer concentration and the flow rate of mobile phase on the enantioseparation were examined to optimize the separation conditions. These may be empolyed to understand the chiral recognition mechanism.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2005年第12期1779-1782,共4页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.39770856)资助项目
关键词
尼卡地平
手性分离
卵类糖蛋白
高效液相色谱
Nicardipine, enantioseparation, ovoglycoprotein, high performance liquid chromatogrpahy